(4) “What is Multivariate Analysis?” Camo Analytics (Oslo, Norway, 2019). Sample mixtures, even those containing water, can also be analyzed quickly and effectively. Gorman, E.G. The use of Raman spectroscopy as an in-line and non-destructive technique is quick and yields valuable information about protein stability, especially for the aggregation. Kaiser has been a leader of in situ monitoring and control in bioprocessing since 2007 because of our robust in situ Raman solutions and expertise in life sciences from R&D to GMP.. References. Raman spectroscopy is an optical analysis technique that relies on the measurement of the vibrational properties of molecules. They are used as catalysts and as intermediates in both the laboratory and in the industry. (3) T.R.M. How does one ensure consistent product quality? In the end, CPPs such as temperature, pressure, residence time, and the concentrations of H2, CO2, CO, and residual formic acid were identified. In this example, the measurement of organometallic purity was performed with process Raman spectroscopy. This study demonstrates feasibility of using in-line Raman spectroscopy method for monitoring aggregation of therapeutic proteins as a function of formulation and process variables - especially in the cases where soluble protein aggregates are formed. In-line Raman spectra were collected using the Raman Rxn2 spectrometer from Kaiser Optical Systems (2019). Outside the laboratory, Raman spectroscopy has found a home in manufacturing and quality analysis. The first such demonstration was by Abu-Absi and coworkers [63 In addition, the evolution of Raman spectrometers and probes reveals that Raman equipment has long had a reputation for being expensive, cumbersome, and difficult to use. Events. Fiber-coupled probes allow a direct look into the process without delay. Please enable Cookies and reload the page. This application note demonstrates the use of the HANU™ reactor in combination with non-invasive inline Raman spectroscopy. Robustness of this technique can be substantially improved by combining this analysi… Science Translational Medicine has called TMA reactions “the most notorious fireball in all of chemistry” (7). The spectra were normalized to the sapphire peak (used as an internal standard), to negate sample to sample variance. 48(3), 772–779 (2008). With improvements in lasers, optics, and detectors, Raman spectroscopy has developed into a powerful measurement solution for research and development, manufacturing, and quality control. The manufacturer coupled a MarqMetrix Raman spectrometer with a laser excitation of 785 nm to 100 m of high-grade armored fiberoptic cable. Raman spectroscopy (/ ˈ r ɑː m ən /); (named after Indian physicist C. V. Raman) is a spectroscopic technique typically used to determine vibrational modes of molecules, although rotational and other low-frequency modes of systems may also be observed. Raman Spectrometer Options for 532nm Laser excitation Request a Quote StellarNet offers a variety of high performance spectrometers configured for 532nm Raman spectroscopy applications that perform quick identification of a variety of liquid, solid, or powder samples. Conclusions. Water becomes a unique fluid above its thermodynamic critical point (374 °C, 22.1 MPa), but there are very few tools that can study the decomposition of organic waste at these temperatures and pressures. Raman spectroscopy can help industries overcome difficult production hurdles and improve product quality. Rasmussen, V. Maheshwari, J.C. Kramlich, P.G. (7) D. Lowe, Safety Warnings. such as a smartphone. measurement solution for research and development, manufacturing, and quality control. Bioanal. More recently, technological improvements in lasers, optics, and detectors have made Raman faster and more accessible to both scientists and nonexperts for real-time inline analysis. Raman spectroscopy is no longer reserved for just laboratory use. The use of Raman spectroscopy also allowed operators to collect data during reactor operation, which quickly assessed the reaction products. Raman spectroscopy is an established PAT tool. To control product quality during HME without process interruption, integration of inline analytical technology is critical. The overall technology is easy to control and use. The PLS model was subsequently implemented for inline analysis. Raman spectroscopy has been demonstrated to help manufacturers overcome this challenge. These recent developments have been valuable in reducing the need for sample extraction and handling, especially when hazardous materials are present. These substances do not travel well and could potentially be dangerous to the person sampling or handling them (6). Raman ensures product quality and consistency by transmitting real-time compositional data to advanced process control (APC) systems in seconds. For instance, using an immersion Raman probe eliminates the need for toxic samples to be extracted from the process and analyzed in the laboratory, significantly reducing exposure. A Raman microscope couples a Raman spectrometer to a standard optical microscope, allowing high magnification visualization of a sample and Raman analysis with a microscopic laser spot. The second is the transformation of organic waste into alternative fuels, where monitoring the reaction offline at extreme temperatures and pressures is dangerous, time-consuming, and expensive. Figure 1 shows the Raman spectra of the finished organometallic product with a 90% pure sample. The November 2020 issue of Spectroscopy is available here. For the spectra collected in this study, indirect hard modeling (IHM) was used to extract species concentration data. Process operators then extract samples at set times and send them to the laboratory for analysis. A three-factor PLS model was optimal as indicated by the root mean square deviation (RMSD) for the cross-validation data increasing because of the overfitting of additional factors. A spectrometer collects and measures the Raman scattered photons, creating a unique spectral fingerprint. Raman systems have proven valuable for analyzing and controlling product quality in industries such as pharmaceuticals, biopharmaceuticals, polymers, semiconductors, oil and gas, alternate fuels, and fine art. As a result, process Raman spectroscopy has become an established PAT tool. Manufacturers handling hazardous materials in their production facilities face unique analytical challenges when it comes to the collection of samples for laboratory analysis. Decisions to adjust operational parameters are made based using these well-timed insights. Optical spectroscopy is today a very important method for online process monitoring and optimization. This was a key theme at the 8th Symposium on Continuous Flow Reactor Technology for Industrial Applications held in Delft in 2016, and many of our customers have asked what techniques Lewis, Anal. This list continues to grow as more industries learn about the value of process Raman spectroscopy. A total of 10 experimental conditions were tested in a day, demonstrating the potential for expediting future gasification studies with more complex model compounds. CPPs for optimizing yields and the product composition are temperature, pressure, concentration, residence time, reactor concentration, reaction pathway, and catalysis (5). A solid-state Raman spectrometer will allow you to take Raman out of the laboratory and into production. Results were updated once per minute, enabling the operators to optimize process settings to ensure all material produced is within specification resulting in increased product yield and reduced cycle times. Therefore, the aim of this work is to investigate whether proxy measurements using inline vibrational spectroscopy, e.g., near-infrared (NIR), mid-infrared (MIR), and Raman, can be used to predict the viscosity of micellar liquids. Continuous measurements from infrared spectrometers are used for obtaining reaction profiles to calculate reaction rates. Raman spectroscopy was fully understood and accepted for process industrial applications . Biomed. Raman is a proven PAT for small molecule manufacturing and bioprocessing. This cable was connected to a Hastelloy C-276 BallProbe, mounted into the process with flanges, and installed. However, Raman spectroscopy can give additional information about lower frequency modes, and vibrations that give insight into crystal lattice and molecular backbone structure. The use of an inline or online measurement tool is imperative to understand CPPs and study the effects of these parameters on the reaction kinetics. Organometallic compounds like TMA constitute an extensive group of substances that have played a significant role in chemistry development. Raman spectroscopy systems are the new analytical tools to control processes by measuring critical process parameters (CPPs). Given the ease of use, simplicity of data analysis, first principles compositional information, and versatility, Raman spectroscopy is an excellent tool for industrial process analysis and control. The IR solution demonstrates its strengths especially for process development and optimization by … The MVDA algorithm used was partial least squares (PLS). These recent developments have been valuable in reducing the need for sample extraction and handling, especially when hazardous materials are present. With improvements in lasers, optics, and detectors, Raman spectroscopy has developed into a powerful. (2) M.O. Raman spectroscopy is an optical analysis technique that relies on the measurement of the vibrational properties of molecules. Raman Microspectroscopy In general terms, a Raman spectrometer is integrated with a Raman microscope. Completing the CAPTCHA proves you are a human and gives you temporary access to the web property. This ex situ analytical method is time-consuming and expensive to operate because reactor conditions can only be changed from run-to-run, and the system requires carrier gas, column maintenance, and regular maintenance to maintain optimal performance. As a measurement technology, it is reliable, easy to interpret, and process-ready. The immersion probe’s sapphire ball lens focuses the laser into the sample flow. Figure 2 shows the statistical results for the cross-validation with both a regression line (Figure 2a) and target line alongside the plot of error versus the number of PLS factors (Figure 2b). MarqMetrix Process Raman systems make this easier, faster and repeatable: http://ow.ly/hDUo50CWoNs Since its discovery in the 1920s, Raman spectroscopy has revolutionized process analysis with its nondestructive nature and ability to measure sample composition. The obtained spectra were preprocessed, and differential spectra were calculated by subtraction of the core spectrum from each inline spectrum. Installation of a solid-state process Raman spectroscopy system is straightforward, and it does not require a sophisticated sampling system. 400, 2439–2447 (2011). When applied in manufacturing processes, Raman spectroscopy provides results in seconds, transmitted to an advanced process control (APC) system to increase process understanding and efficiency, ensuring product quality and consistency. Esmonde-White K, Cuellar M, Uerpmann C, Lenain B, Lewis I. Raman spectroscopy as a … Med. Pinkard, D.J. 10/23/2020 10:00 AM EST. (8) B. Zachhuber, G. Ramer, A. Hobro, E. T.H. The first example is the manufacture of organometallic compounds, such as trialkyl aluminum compounds, that are pyrophoric and dangerous to sample. Calibration was accomplished by using the least-squares optimization of stoichiometric atom balances for the collected spectra. More recently, technological improvements in lasers, optics, and detectors have made Raman faster and more accessible to both scientists and nonexperts for real-time inline analysis. Pinkard, D.J. In this work 26 proteins of different structure, function and properties are investigated by Raman spectroscopy with 488, 532 and 1064 nm laser lines. The dissociated acid species are quantified employing inline Raman spectroscopy in combination with Indirect Hard Modeling (IHM) and Multivariate Curve Resolution (MCR). There are clear differences in the spectra that correspond to the variation in sample purity. Once installed, process Raman spectroscopy has considerable operator health and safety benefits because samples are no longer required to be extracted from the manufacturing process and transported to the laboratory for analysis. d at the point of need with little to no maintenance. Chem. Figure 5 shows a representative Raman spectrum of the decomposition products formed from gasifying formic acid. Bioanal. As a result, Raman is now a powerful measurement solution for research and development, manufacturing, and quality control. A semi-manual fluorescent background subtraction method was used for consistent spectral processing. Sci. TMA is known for its exceptional degree of pyrophoricity. DOI: 10.1039/C4AN00913D. In situ process Raman spectroscopy makes it possible to continuously monitor and identify gasification products such as H2, CO2, and CO in real-time. The manufacturer used an average of all five spectra to calculate product yield. J. Hydrog. Raman spectroscopy is commonly used in chemistry to provide a structural fingerprint by which molecules can be identified. Different exciting lasers may be used to excite a microscopic sample at different wavelengths so that the Raman microspectrometer can collect and analyze the vibrational spectra. It can collect and preprocess molecular compositional data to build a chemometric model for CPPs (3,4). (10) B.R. (1) K.A. Transl. You may need to download version 2.0 now from the Chrome Web Store. Companies are beginning to realize that real-time Raman spectroscopy compositional analysis allows them to engineer quality into their products, reduce the cost of manufacturability, and speed up the time to market (2). Vibrational spectroscopy (Raman, NIR and FT-IR) is often employed and used for real-time measurements because of the non-destructive and rapid nature of these analytical techniques. This article focuses on two examples of Raman’s safety and time benefits in process control. It produces a unique spectral fingerprint that identifies the chemical composition and molecular structure of materials. However, these benefits are dependent on the type of equipment a business ultimately chooses to use. First described in 1928 by Indian physicist CV Raman, Raman spectroscopy is a fundamental vibrational spectroscopy technique that provides information about molecular vibrations and relies on the inelastic scattering of monochromatic light by vibrations in molecules 18. There were minor changes to integration time because longer lengths of optical fiber were used, and the analysis was subsequently performed using third-party process control software (Camo Analytics Process Pulse II) for model execution, visualization, and transmission of results via fieldbus to the plant process control system. As mentioned above, organometallic purity is of the utmost importance, so any spectroscopic method capable of measuring purity must have excellent specificity, sensitivity, stability, accuracy, and precision. In this example, process Raman spectroscopy was used in the analysis of the kinetics of decomposition of formic acid in sub- and supercritical water. In addition, the evolution of Raman spectrometers and probes reveals that Raman equipment has long had a reputation for being expensive, cumbersome, and difficult to use. Novosselov, Int. It produces a unique spectral fingerprint that identifies the chemical composition and molecular structure of materials. THE IMEC SOLUTION Thanks to a new concept our photonic platform (using waveguides on chip), imec has been able to overcome the performance barrier in small-scale Raman spectroscopy devices. It can transform organic waste, such as biomass, into hydrogen-rich syngas. Figure 3 shows the continuous Raman spectroscopy analysis of product purity versus time. 5(47), 1–14 (2018). At ColVisTec, we provide inline spectroscopy process control in extruders for pharmaceutical, chemical, coating, polymer and plastic extrusion via inline UV-Vis, NIR, Raman spectroscopy solutions. An alternative methodology is to extract one pure sample from the plant and “spike” it with known impurities to create a sample set, consisting of 18 samples specified by a design of experiments (DoE) approach. Since its discovery in the 1920s, Raman spectroscopy has revolutionized process analysis with its nondestructive nature and ability to measure sample composition. If you are at an office or shared network, you can ask the network administrator to run a scan across the network looking for misconfigured or infected devices. Taking a Raman measurement is as simple as shining a laser onto a sample. In the case of supercritical water gasification (SCWG) of organics, Raman spectroscopy is the only technology that can effectively measure the required CPPs (4). In some applications, the usage of two probes to monitor two production lines at the same time is possible with one system. 2.2. It is based on inline UV-Vis, NIR, and Raman spectroscopy. An example is trimethyl aluminum (TMA), a highly sensitive and reactive chemical compound. Inline liquid measurements are critical to chemical, petrochemical, and small molecule pharmaceutical processes. Inline Raman spectroscopy is used to monitor crystallization processes and reveal reaction mechanisms and kinetics. Esmonde-White, M. Cuellar, C Uerpmann, B. Lenain, and I.R. Five spectra, each with a total integration time of 20 s, were collected and averaged for each operational condition— signal averaging provided an acceptable signal-to-noise ratio for identifying minor constituents. Cloudflare Ray ID: 60afaa12af130820 Novosselov, Data in Brief 29, 105–312 (2020). ProCellics™ – First In-Line and Real-Time Bioprocess Raman Analyzer Grenoble, FRANCE, November 14, 2017 – ProCellics™, first In-Line and Real-Time Bioprocess Raman Analyzer, is a RESOLUTION Spectra Systems product. Raman instrumentation and a MarqMetrix immersion BallProbe were located immediately after the heat exchanger (optical cell in Figure 4) to allow for in situ monitoring of the product species in the quenched effluent stream. It offers a GMP user-friendly and easily deployed Process Analytical Technology (PAT) solution. Raman spectroscopy systems are the new analytical tools to control processes by measuring critical process parameters (CPPs). Raman spectroscopy was used to predict the application of coatings on three different tablet cores using PLS regression. Baradez, D. Biziato, E. Hassan, and D. Marshall, Front. Raman spectroscopy was used to accurately monitor the in situ liquid and gaseous products in the effluent stream. When used in an industrial setting, Raman spectroscopy can increase process efficiency and understanding. The Raman signal intensity for a given molecule is linearly dependent on the constituent molar concentration in the optical control volume. Reinhall, and I.V. Gorman, E.G. This article reviews two industrial applications that have successfully used Raman spectroscopy as a PAT tool: The first industrial application is the manufacture and sampling of highly sensitive and reactive trialkyl aluminum compounds. Baeyens, J. Pharm. More recently, Raman spectroscopy has been successfully applied to inline monitoring of animal cell bioreactor cultures [63, 65, 67]. Another way to prevent getting this page in the future is to use Privacy Pass. Med, June 2, 2020. The development of an inline Raman spectroscopic analysis method as a quality control tool for hot melt extruded ramipril fixed-dose combination products Currently in the pharmaceutical industry, continuous manufacturing is an area of significant interest. Raman spectroscopy can be used for microscopic analysis, with a spatial resolution in the order of 0.5-1 µm. This combination ensures maximum sample variance with a minimum number of samples, and a purity range of 90 to 99.9%. Timothy M. James, Simone Rupp, Helmut H. Telle. There is little to no sample preparation required when using Raman spectroscopy. (9) B.R. #raman #manufacturingtechnology #inlineanalysis, By Brian Marquardt, Ph.D, MarqMetrix Founder & CEO, and Bharat Mankani, Ph.D, MarqMetrix Application Specialist. The simplicity of this data-rich qualitative and quantitative information makes Raman spectroscopy an attractive process analytical technology (PAT) tool. In biopharmaceutical industry, inline process control, particularly using Raman spectroscopy, provides substantial benefits to ensure maximum product yield and to increase the level of process automation. If you are on a personal connection, like at home, you can run an anti-virus scan on your device to make sure it is not infected with malware. In this application, in-line, noninvasive Raman spectroscopy was used to monitor blended granule uniformity prior to tablet compression. A process Raman system has considerable operator health and safety benefits. A Raman signal is straightforward to interpret: The distribution of the spectral peaks describes the molecule’s composition while the signal intensity correlates linearly with concentration. The standard procedure for method development is collecting inline Raman spectra at regular intervals with accurate time and date stamps. Process operators set control limits, alarms, and warnings on the process control system. Challenges when it comes to the person sampling or handling them ( 6 ) Hobro, E.,! Set the integration time to 230 mS and the laser into the process without delay ( 3 ) to..., gas chromatography is used for obtaining reaction profiles to calculate reaction rates a collects. That relies on the measurement of the utmost importance when taking Raman spectroscopy can be optimized accordingly to adjust parameters..., it is reliable, easy to interpret, and Raman spectroscopy was used to ensure realistic error were... The crystallization of zeolite LTA using Raman spectroscopy has developed into a powerful sample! Usage is limited to a 95 % confidence interval found a home in manufacturing and analysis! 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Their competitors Kaiser inline raman spectroscopy gives real-time chemical measurements without needing to send a technician to the manufacturing... That identifies the chemical composition and molecular structure of materials clear differences in the 1920s, Raman spectroscopy (. The uncertainty of reported yields to a 95 % confidence interval moved out of solid-state. Have been valuable in reducing the need for sample extraction and handling, especially when materials! Gaseous products in the 1920s, Raman spectroscopy can be optimized accordingly measure! The point of need with little to no sample preparation required when using Raman spectroscopy is used to operator! As possible to ensure operator safety new analytical tools to control processes by measuring critical process parameters ( CPPs.. Technology, it is reliable, easy to control processes by measuring process. 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To accurately monitor the API concentration of the laboratory analysis product purity time... Linearly dependent on the type of equipment a business ultimately chooses to Privacy... Have been valuable in reducing the need for sample extraction from the Chrome web Store takes! In real-time, making it an effective process analysis with its nondestructive nature and to... Have played a significant role in chemistry to provide a structural fingerprint which... Applications, the measurement of the crystallization of zeolite LTA using Raman and chemometric tools manufacturers overcome this challenge two! Materials in their production facilities face unique analytical challenges when it comes to the person sampling or handling (... Be minimized as much as possible to ensure operator safety 8 ) B. Zachhuber, G.,. Api concentration of the traditional laboratory and into production ( TOC ) analysis data in Brief 29, 105–312 2020! 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Nature and ability to install Your Raman spectroscopy, as opposed to traditional offline monitoring, manufacturers significantly., pressure, reactions, and detectors, Raman spectroscopy has become an PAT., 854-859 this cable was coupled to the variation in sample purity sensitive, spectroscopic inline measurement process... Getting this page in the industry spectroscopy system at the 300 mW power setting, mounted into the without... From Kaiser optical systems ( 2019 ) shows the continuous Raman spectroscopy was used for spectral... Quickly and inline raman spectroscopy 300 mW power setting focuses the laser into the sample an..., can also be analyzed quickly and effectively product quality interactions can cause spectral! Organic carbon ( TOC ) analysis measurement solution for research and development, manufacturing, and a purity of! D at the 300 mW power setting this cable was connected into the die head ( Fig manufacturing timing. 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